CN104267022B - Cross sensitivity material of Ammonia in Air and benzene and preparation method thereof - Google Patents
Cross sensitivity material of Ammonia in Air and benzene and preparation method thereof Download PDFInfo
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- CN104267022B CN104267022B CN201410460628.XA CN201410460628A CN104267022B CN 104267022 B CN104267022 B CN 104267022B CN 201410460628 A CN201410460628 A CN 201410460628A CN 104267022 B CN104267022 B CN 104267022B
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Abstract
The present invention relates to the cross sensitivity material of a kind of Ammonia in Air and benzene, is by graphene-supported gross mass mark 2-4%Pd, 10-14%Bi
2o
3, 5-11%SnO
2and 10-20%V
2o
5the composite powder material of composition.Its preparation method is: add in the concentrated sulphuric acid by native graphite and ammonium phosphate, and reacted much filtrate uses potassium dichromate concentrated sulfuric acid solution and aqueous hydrogen peroxide solution process successively, obtains graphene oxide; Palladium chloride, bismuth salt, pink salt and vanadic salts are dissolved in aqueous hydrochloric acid solution altogether, after adding ethylenediamine tetraacetic acid, add graphene oxide, after adding hydrazine hydrate aqueous solution reaction, through ageing, filtration, drying and roasting, obtain cross sensitivity material.The ammonia using sensitive material provided by the present invention to make and benzene catalytic luminescence sensor, have the wider range of linearity, good selectivity and higher sensitivity, can ammonia in on-line monitoring air and benzene and not by the impact of coexisting substances.
Description
Technical field
The present invention relates to a kind of for cross sensitivity material of monitoring Ammonia in Air and benzene and preparation method thereof, especially graphene-supported Bi atom doped by palladium
2o
3, SnO
2and V
2o
5the composite sensitive material of composition, belongs to field of sensing technologies.
Background technology
Ammonia (NH
3) be a kind of alkalescence, colourless, the gas with intense stimulus smell, the ammonia in air is often attracted in human body skin mucous membrane, eye conjunctiva and respiratory tract mucosa because of soluble in water.When Ammonia in Air gas concentration is 0.5mg/m
3time people can be made to feel penetrating odor; When Ammonia in Air gas concentration is more than 80mg/m
3time, people can be made in the short time to occur shedding tears, pharyngalgia, cough, uncomfortable in chest, expiratory dyspnea, and with dizziness, headache, Nausea and vomiting, the symptom such as weak, also can there is pulmonary edema and respiratory disease in serious.People live in the ammonia environment of low concentration for a long time, can benumb respiratory tract cilium and infringement mucous epithelium tissue gradually, make sex pheromone be easy to invade, weaken the resistibility of health to disease.
Benzene is a kind of industrial chemicals with aromatic odor, and Chronic Benzene Poisoning mainly has spread effect to skin, eyes and the upper respiratory tract; Frequent Contact benzene, skin can because of degreasing desiccation furfur, some appearance allergic eczemas; Long-term suction benzene can cause alpastic anemia.
In recent years, because the use of interior decoration and all kinds of Modern Live articles for use makes room air pollution be on the rise.The major pollutants of room air have: ammonia, benzene, formaldehyde and radon gas, and wherein the exceeding standard rate of ammonia and benzene is all higher.Recently, national departments concerned has spot-check the newly-built high-grade office building in Beijing and home dwelling community, detects its IAQ (indoor air quality), and in discovery room air, ammonia and benzene all exceed standard and reaches more than 60%; Spot-check its house decorative material, result disqualification rate is more than 50%.Human health in air quality serious threat.
The conventional sense means of ammonia mainly contain: spectrophotometric method, vapor-phase chromatography, liquid phase chromatography and electrochemical process etc.These method sensitivity are all higher, but complicated operation, must complete in laboratory, cannot on-the-spotly realize.The on-site measurement method of ammonia mainly contains detector tube colourimetry, this method stability and sensitivity all not enough, the Accurate Determining of micro-ammonia cannot be completed.The method measuring benzene mainly contains photometry, electrochemical process, chromatography, chemoluminescence method, makings Liquid Chromatography/Mass Spectrometry and the chromatography of ions etc.These methods all need preconcentration and suitably process ability to complete mensuration by analytical instrument, and therefore length consuming time is not easily on-the-spot realizes.Being entitled as in the paper of " nano composite material catalytic luminescence method measures the benzene homologues in air " that inventor delivered on " assay office " in 2006 uses nanosized copper ferromanganese (atomic ratio 4: 3: 1) composite oxides as sensitive material, can on-line checkingi 1 ~ 80mg/m
3benzene homologues, detection limit can reach 0.5mg/m
3but formaldehyde, methyl alcohol, ethanol and the acetone mensuration to benzene homologues has certain interference; Patent of invention 200910223546.2 discloses a kind of nano sensitive material of monitoring benzene homologues, and the sensor utilizing this material to prepare can monitor the micro-benzene in air, but formaldehyde, methyl alcohol, sulfuretted hydrogen and acetic acid etc. also have response signal; Patent of invention 200710306935.2 discloses a kind of nano composite oxide sensitive material of ammonia, and the ammonia gas sensor PARA FORMALDEHYDE PRILLS(91,95), methyl alcohol and the ethanol that utilize this material to prepare also have response signal; These all show that the selectivity of sensitive material has much room for improvement.
Summary of the invention
The object of the invention is the deficiency overcoming conventional art, provide a kind of has catalytic luminescence cross sensitivity material and preparation method thereof compared with high selectivity to ammonia and benzene simultaneously.The monitoring ammonia made of this sensitive material and the gas sensor of benzene, can Ammonia at the scene fast, in Accurate Determining air and benzene and not by the interference of other concurrent.
Sensitive material of the present invention is the graphene-supported Bi atom doped by Pd
2o
3, SnO
2and V
2o
5the composite powder material of composition, its preparation method is:
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 40-50 DEG C, and constant temperature stirs the ammonium phosphate slowly added after 2-3 hour with the weight such as native graphite, and continue constant temperature and stir 3-4 hour, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 50-55 DEG C of temperature, slowly adding massfraction is that the aqueous hydrogen peroxide solution of 15-25% is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, bismuth salt, it be 35 DEG C of massfractions is in the aqueous hydrochloric acid solution of 10% that pink salt and vanadic salts are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, keep the continuous dispersed with stirring of temperature 2 hours, add the hydrazine hydrate aqueous solution that massfraction is 25%, continuation stirring still aging 2-5 hour after 1 hour, sedimentation and filtration to be placed in drying box dry 5-10 hour at 95-110 DEG C of temperature, after abundant grinding, 300-330 DEG C is warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2-3 hour, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
Wherein, bismuth salt is the anhydride of bismuth acetate, bismuth oxalate, bismuth nitrate, bismuth sulfate, bismuth phosphate and bismuth trichloride or the potpourri of one or more of hydrate, pink salt is tin chloride, stannous chloride, the sub-tin of nitric acid and the anhydride of stannous sulfate or the potpourri of one or more of hydrate, and vanadic salts is ammonium metavanadate.
When the obtained each constituent mass mark of composite powder material meets Pd (2-4%), Bi
2o
3(10-14%), SnO
2(5-11%), V
2o
5(10-20%) time with C (50-70%), for there is very high sensitivity and selectivity as the cross sensitivity material of monitoring Ammonia in Air and benzene.
Embodiment
Embodiment 1
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 42 DEG C, and constant temperature slowly adds the ammonium phosphate with the weight such as native graphite after stirring 2 hours, and continue constant temperature and stir 3 hours, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 55 DEG C of temperature, slowly adding massfraction is that 15% aqueous hydrogen peroxide solution is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, bismuth acetate, it be the massfraction of 35 DEG C is in the aqueous hydrochloric acid solution of 10% that five water tin chlorides and ammonium metavanadate are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, the continuous dispersed with stirring of temperature is kept after 2 hours, to add the hydrazine hydrate aqueous solution that massfraction is 25%, continue stirring after 1 hour still aging 3 hours, sedimentation and filtration to be placed in drying box at 95 DEG C of temperature dry 10 hours, after abundant grinding, 325 DEG C are warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2.5 hours, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
Analyze: carry out constituent analysis to composite powder material, recording mass percent is 3%Pd, 13.8%Bi
2o
3, 5.8%SnO
2, 19.5%V
2o
5be C with all the other.
Application: measure the ammonia in air and benzene using this powder body material as sensitive material, the range of linearity is ammonia 0.7-63mg/m
3with benzene 0.5-75mg/m
3, detect and be limited to ammonia 0.2mg/m
3with benzene 0.2mg/m
3, concurrent does not disturb.
Embodiment 2
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 45 DEG C, and constant temperature slowly adds the ammonium phosphate with the weight such as native graphite after stirring 2.5 hours, and continue constant temperature and stir 3.5 hours, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 54 DEG C of temperature, slowly adding massfraction is that 17% aqueous hydrogen peroxide solution is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, seven water bismuth oxalates, it be the massfraction of 35 DEG C is in the aqueous hydrochloric acid solution of 10% that stannous chloride dihydrate and ammonium metavanadate are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, the continuous dispersed with stirring of temperature is kept after 2 hours, to add the hydrazine hydrate aqueous solution that massfraction is 25%, continue stirring after 1 hour still aging 4 hours, sedimentation and filtration to be placed in drying box at 98 DEG C of temperature dry 9 hours, after abundant grinding, 320 DEG C are warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2 hours, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
Analyze: carry out constituent analysis to composite powder material, recording mass percent is 2.2%Pd, 13.3%Bi
2o
3, 7.2%SnO
2, 18.2%V
2o
5be C with all the other.
Application: measure the ammonia in air and benzene using this powder body material as sensitive material, the range of linearity is ammonia 1.1-86mg/m
3with benzene 0.6-78mg/m
3, detect and be limited to ammonia 0.4mg/m
3with benzene 0.2mg/m
3, concurrent does not disturb.
Embodiment 3
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 47 DEG C, and constant temperature slowly adds the ammonium phosphate with the weight such as native graphite after stirring 3 hours, and continue constant temperature and stir 3.9 hours, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 53 DEG C of temperature, slowly adding massfraction is that 20% aqueous hydrogen peroxide solution is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, five water bismuth nitrates, bismuth sulfate, it be the massfraction of 35 DEG C is in the aqueous hydrochloric acid solution of 10% that the sub-tin of nitric acid and ammonium metavanadate are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, the continuous dispersed with stirring of temperature is kept after 2 hours, to add the hydrazine hydrate aqueous solution that massfraction is 25%, continue stirring after 1 hour still aging 4.5 hours, sedimentation and filtration to be placed in drying box at 100 DEG C of temperature dry 8 hours, after abundant grinding, 315 DEG C are warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2 hours, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
Analyze: carry out constituent analysis to composite powder material, recording mass percent is 2.8%Pd, 12.5%Bi
2o
3, 8.8%SnO
2, 17.1%V
2o
5be C with all the other.
Application: measure the ammonia in air and benzene using this powder body material as sensitive material, the range of linearity is ammonia 0.9-71mg/m
3with benzene 0.5-73mg/m
3, detect and be limited to ammonia 0.3mg/m
3with benzene 0.1mg/m
3, concurrent does not disturb.
Embodiment 4
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 49 DEG C, and constant temperature slowly adds the ammonium phosphate with the weight such as native graphite after stirring 2.8 hours, and continue constant temperature and stir 3.2 hours, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 52 DEG C of temperature, slowly adding massfraction is that 22% aqueous hydrogen peroxide solution is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, bismuth phosphate, it be the massfraction of 35 DEG C is in the aqueous hydrochloric acid solution of 10% that stannous sulfate and ammonium metavanadate are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, the continuous dispersed with stirring of temperature is kept after 2 hours, to add the hydrazine hydrate aqueous solution that massfraction is 25%, continue stirring after 1 hour still aging 2.5 hours, sedimentation and filtration to be placed in drying box at 105 DEG C of temperature dry 7 hours, after abundant grinding, 310 DEG C are warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2.5 hours, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
Analyze: carry out constituent analysis to composite powder material, recording mass percent is 3.5%Pd, 11.6%Bi
2o
3, 9.5%SnO
2, 15.2%V
2o
5be C with all the other.
Application: measure the ammonia in air and benzene using this powder body material as sensitive material, the range of linearity is ammonia 1.0-77mg/m
3with benzene 0.8-83mg/m
3, detect and be limited to ammonia 0.3mg/m
3with benzene 0.3mg/m
3, concurrent does not disturb.
Embodiment 5
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 50 DEG C, and constant temperature slowly adds the ammonium phosphate with the weight such as native graphite after stirring 2.1 hours, and continue constant temperature and stir 3.8 hours, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 51 DEG C of temperature, slowly adding massfraction is that 24% aqueous hydrogen peroxide solution is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, bismuth acetate, bismuth trichloride, stannous chloride dihydrate, it be the massfraction of 35 DEG C is in the aqueous hydrochloric acid solution of 10% that the sub-tin of nitric acid and ammonium metavanadate are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, the continuous dispersed with stirring of temperature is kept after 2 hours, to add the hydrazine hydrate aqueous solution that massfraction is 25%, continue stirring after 1 hour still aging 3.5 hours, sedimentation and filtration to be placed in drying box at 108 DEG C of temperature dry 6 hours, after abundant grinding, 305 DEG C are warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 3 hours, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
Analyze: carry out constituent analysis to composite powder material, recording mass percent is 3.8%Pd, 10.2%Bi
2o
3, 10.8%SnO
2, 11.3%V
2o
5be C with all the other.
Application: measure the ammonia in air and benzene using this powder body material as sensitive material, the range of linearity is ammonia 0.8-65mg/m
3with benzene 0.7-72mg/m
3, detect and be limited to ammonia 0.2mg/m
3with benzene 0.3mg/m
3, concurrent does not disturb.
Claims (3)
1., for monitoring a cross sensitivity material for Ammonia in Air and benzene, it is characterized in that by graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition, wherein the mass percent scope of each component is 2-4%Pd, 10-14%Bi
2o
3, 5-11%SnO
2, 10-20%V
2o
5and 57.9-70%C, its preparation method is:
(1) with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 40-50 DEG C, and constant temperature stirs the ammonium phosphate slowly added after 2-3 hour with the weight such as native graphite, and continue constant temperature and stir 3-4 hour, much filtrate is also washed to neutrality by suction filtration; Filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 50-55 DEG C of temperature, slowly adding massfraction is that the aqueous hydrogen peroxide solution of 15-25% is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide;
(2) by palladium chloride, bismuth salt, it be 35 DEG C of massfractions is in the aqueous hydrochloric acid solution of 10% that pink salt and vanadic salts are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, keep the continuous dispersed with stirring of temperature 2 hours, add the hydrazine hydrate aqueous solution that massfraction is 25%, continuation stirring still aging 2-5 hour after 1 hour, sedimentation and filtration to be placed in drying box dry 5-10 hour at 95-110 DEG C of temperature, after abundant grinding, 300-330 DEG C is warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2-3 hour, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
2. a kind of cross sensitivity material for monitoring Ammonia in Air and benzene according to claim 1, it is characterized in that described bismuth salt is the anhydride of bismuth acetate, bismuth oxalate, bismuth nitrate, bismuth sulfate, bismuth phosphate and bismuth trichloride or the potpourri of one or more of hydrate, pink salt is tin chloride, stannous chloride, the sub-tin of nitric acid and the anhydride of stannous sulfate or the potpourri of one or more of hydrate, and vanadic salts is ammonium metavanadate.
3. one kind for monitoring the preparation method of the cross sensitivity material of Ammonia in Air and benzene, it is characterized in that with continuous stirring native graphite slowly being added temperature is in the concentrated sulphuric acid of 40-50 DEG C, constant temperature stirs the ammonium phosphate slowly added after 2-3 hour with the weight such as native graphite, continue constant temperature and stir 3-4 hour, much filtrate is also washed to neutrality by suction filtration, filter cake being added massfraction is in the potassium dichromate concentrated sulfuric acid solution of 10%, stir continuously after 1.5 hours under keeping 50-55 DEG C of temperature, slowly adding massfraction is that the aqueous hydrogen peroxide solution of 15-25% is to bubble-free, continue constant temperature and stir 1 hour, much filtrate is also washed to neutrality by suction filtration, obtains graphene oxide, by palladium chloride, bismuth salt, it be 35 DEG C of massfractions is in the aqueous hydrochloric acid solution of 10% that pink salt and vanadic salts are dissolved in temperature altogether, sonic oscillation is to clarification, appropriate ethylenediamine tetraacetic acid is added under high-speed stirred, add graphene oxide subsequently, keep the continuous dispersed with stirring of temperature 2 hours, add the hydrazine hydrate aqueous solution that massfraction is 25%, continuation stirring still aging 2-5 hour after 1 hour, sedimentation and filtration to be placed in drying box dry 5-10 hour at 95-110 DEG C of temperature, after abundant grinding, 300-330 DEG C is warming up to the speed being no more than 5 DEG C per minute in chamber type electric resistance furnace, keep this temperature calcination 2-3 hour, obtain graphene-supported Pd, Bi
2o
3, SnO
2and V
2o
5the composite powder material of composition.
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CN104849402B (en) * | 2015-04-20 | 2016-11-23 | 北京联合大学 | A kind of cross sensitivity material of benzene, toluene and ethylbenzene |
CN109490372B (en) * | 2018-11-30 | 2020-11-17 | 北京联合大学 | Catalytic luminous sensitive material of ethanol |
CN110455978B (en) * | 2019-06-30 | 2021-09-14 | 北京联合大学 | Benzene and ammonia low-temperature catalytic luminescence cross-sensitive material |
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US7074319B2 (en) * | 2002-12-11 | 2006-07-11 | Delphi Technologies, Inc. | Ammonia gas sensors |
JP2011047756A (en) * | 2009-08-26 | 2011-03-10 | Ngk Spark Plug Co Ltd | Ammonia gas sensor |
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CN103792227B (en) * | 2014-01-22 | 2017-02-15 | 北京联合大学生物化学工程学院 | Nano composite oxide sensitive material for formaldehyde and benzene |
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